US4211799A - Methods for making flocculation-resistant citrus juice - Google Patents

Methods for making flocculation-resistant citrus juice Download PDF

Info

Publication number
US4211799A
US4211799A US05/944,697 US94469778A US4211799A US 4211799 A US4211799 A US 4211799A US 94469778 A US94469778 A US 94469778A US 4211799 A US4211799 A US 4211799A
Authority
US
United States
Prior art keywords
juice
bentonite
calcium
turbid
sodium
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
US05/944,697
Other languages
English (en)
Inventor
Ekkehard Grampp
Reinhold Schmitt
Helmut Uhlig
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Roehm GmbH Darmstadt
Original Assignee
Roehm GmbH Darmstadt
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Roehm GmbH Darmstadt filed Critical Roehm GmbH Darmstadt
Application granted granted Critical
Publication of US4211799A publication Critical patent/US4211799A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/70Clarifying or fining of non-alcoholic beverages; Removing unwanted matter
    • A23L2/84Clarifying or fining of non-alcoholic beverages; Removing unwanted matter using microorganisms or biological material, e.g. enzymes

Definitions

  • the present invention relates to methods for making citrus juice which is resistant to flocculation on storage.
  • Citrus juices are turbid by nature.
  • the turbidifying materials are suspended by pectins, among other substances.
  • the materials settle by themselves only very slowly and, also, cannot be filtered out.
  • the pectins hydrolyze under the influence of the acids and enzyme systems naturally contained within the juice and gradually lose their effect of stabilizing the turbidifying materials so that the latter settle.
  • naturally turbid citrus juices are not suited for direct use after they have been in storage for long periods.
  • the gross turbidifying materials can be largely separated by centrifugation. However, the formation of clouds or floccules occurs again after pasteurization if the juice is stored for a long time.
  • the object of the present invention is to impart a flocculation-resistant, storage-stable property to naturally turbid citrus juice having a pH value under 2.5 in a short period of time.
  • This goal can be accomplished either by stabilizing the natural turbidity which is present so that it remains resistant to flocculation over long periods of storage or, on the other hand, by fully clarifying the juice in a short period of time. In both cases, a storage time of several months at room temperature should not generate the formation of clouds or floccules.
  • both goals can be reached according to choice.
  • Basic to the discovery is the recognition that strongly acid citrus juices contain two kinds of turbidifying materials having differing properties.
  • One kind of turbidifying material is, as in other fruit juices, stabilized by pectins and precipitates if the pectins are decomposed.
  • the second kind of turbidifying material is self-stabilized. Apparently, these latter turbidifying materials are carried along during the gradual settling out of the first-mentioned turbidifying materials upon self-induced pectin degradation.
  • these turbidifying materials of the second kind are completely stable also in the absence of pectin if one removes the pectin-stabilized turbidities.
  • they can be flocculated out surprisingly easily by means of a silica sol, whereas this agent exercises no influence on the pectins-stabilized turbidities.
  • the pectin-dependent portion of the turbidifying materials separates by flocculation and, as for other juices, can be separated by decantation. The remaining turbidity is resistant to further flocculation.
  • a clear juice stable against subsequent turbidification is prepared by the post-treatment of the turbid juice so obtained with a silica sol in a manner which is described in more detail later herein.
  • all strongly acid citrus juices having a pH value under 2.5 can be treated, such as lemon, lime, bergamot, and grapefruit juice, as well as the re-diluted juices obtained from the corresponding concentrates.
  • Weakly acid citrus juices, for example orange juice are also clarified according to the measures according to the present invention. However, such clarification can be carried out equally well with other pectinases and by modified procedural techniques.
  • pectinases of the polygalacturonase-pectinesterase type. These are characterized by a high pectolytic activity below pH 2.5.
  • pectinase is here intended the total enzyme complex produced by whatever microorganism is involved, which complex may possibly include accompanying enzymes which are essential for the total effect.
  • Enzyme complexes of the type used according to the invention are obtained from mold fungus cultures, for example those of Aspergillus niger, Aspergillus saitoi, and Aspergillus wentii, or Sclertonia libertiana.
  • a suitable commercially-available product is "Rohapect C" (Rohm GmbH).
  • the pectinases of the transeliminase type which are usually employed in the clarification of fruit juice, particularly for apple juice, are unsuited for the process of the invention.
  • known methods of pectinase treatment in which a visible destabilization of the turbid matter and the formation of clouds or floccules occur on pectin degradation, only a portion of the turbidifying materials are destabilized by the process of the invention. Since, after the separation of this portion, a considerable portion of the turbid material is still always present and, further, also does not separate further, the pectinase treatment according to the present invention cannot simply be compared with a conventional clarification method.
  • the method of the invention is also distinguished from conventional clarification methods in the conditions under which the enzyme acts. Whereas pectinases are mostly permitted to operate at 40° to 50° C. for one to two hours, a temperature of 30° C. may not be exceeded in the process of the invention. The preferred temperature is from 15° to 25° C. The period of activity is extended for such a time until the alcohol test for pectin is negative. In general, this requires at least four hours, preferably 12 to 24 hours. For the alcohol test, a sample of the juice is combined with an equal volume of ethanol. If a gel is still formed thereby, which gel floats, treatment is continued.
  • the amount of enzyme required is from 50 g to 200 g for 1000 liters of juice if the enzyme is of commercial quality having about 700 PGU/mg. Enzyme products having more than 700 PGU/mg are employed in a correspondingly smaller amount and vice versa.
  • the standard pectin solution is made by mixing 0.71 g of pectin with 1 ml of ethanol and dissolving the mixture in water. After the addition of 20 ml of a citric acid buffer solution at pH 4.0, the solution is diluted to 100 ml and is filtered after standing for 12 hours. 15 ml of the solution contain 100 mg of pertin.
  • the turbidifying portion which is destabilized by the pectinase treatment is separated in the usual fashion by decantation. This includes all conventional methods for the separation of the residue from the settled turbid material, for example also centrifugation.
  • the use of sodium-calcium-bentonite (which is obtained from natural bentonite by a partial exchange of Ca-ions for Na-ions) as a decantation auxiliary is advantageous.
  • the bentonite is employed in small amounts in the preparation of turbid citrus juices, for example 0.1 to 1 kg per 1000 liters of juice.
  • Na-Ca-bentonite is added to the juice in a considerable amount, namely from 1 to 4 kg per 1000 liters of juice.
  • Re-diluted concentrates can, for the most part, already be obtained in clear condition by filtration after further addition of a silica sol and a short period of standing.
  • the amount of silica sol (calculated as a sol having 15% dry solids content) is about one half of the amount of bentonite.
  • a period of at least a half hour preferably at least a complete hour, should extend between the addition of the bentonite and that of the silica sol. In this period the juice should be stirred at least from time to time.
  • silica sol a product of the quality obtained by the hydrolysis of silicon tetrachloride in the vapor phase with subsequent dispersion in water is preferably employed.
  • a typical product of this kind has a specific surface area of 170 m 2 /g.
  • the clear juice can be obtained by filtration without difficulty and is then suitable for the preparation of soft drinks, scents, candies, and the like.
  • the juice can be concentrated from a value of, generally, 7°-9° Brix to about 70° Brix.
  • the juice is recovered from freshly-harvested lemons using a ball press. Coarse turbidifying particles and fibers are removed from the juice so obtained using a finisher.
  • the juice contains demonstrable amounts of pectin.
  • the juice temperature is about 20° C. 100 g of a pectinase preparation from Asp. niger (700 PGU/mg) are added to 1000 liters of juice and distributed well throughout. After a period of 20 hours, the pectin is decomposed and cannot be found employing the alcohol test.
  • Freshly pressed lemon juice with demonstrable amounts of pectin is freed of a portion of the turbidifying material by means of a centrifuge. Subsequently, 200 g of a pectinase preparation from Asp. niger (1000 PGU/mg) is added to 1000 liters of this juice at a temperature of 25° C. and mixed. After five hours operating temperature no pectin can any longer be found.
  • the floccules which form are left to stand for one hour.
  • the juice is briefly stirred once more and then again left to stand. After five hours of standing, the floccules have settled and the supernatant juice is clear. It is drawn off, filtered and thickened in a vacuum evaporator to form a clear concentrate.
  • the clear filtered juice so obtained is worked up into a beverage, pasteurized, and bottled.
  • the turbidifying particles destablized by the degenerated pectin, are removed using a centrifuge. Colloidally divided fine turbidifying material remains in the juice. After pasteurization and bottling, the juice remains homogeneously turbid and forms no precipitate during subsequent storage.
  • Pectin-free lemon juice prepared according to Example 4 is combined with 0.5 kg of pre-swollen sodium-calcium-bentonite per 1000 liters.
  • the bentonite adsorbs a portion of the primary de-stabilized turbidity and settles within 10 hours.
  • the slightly turbid supernatant juice is drawn off and pasteurized. After conversion into a turbid beverage, it is pasteurized and bottled. On storage, the beverage has no tendency to form floccules or a precipitate and remains homogeneously turbid.

Landscapes

  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Microbiology (AREA)
  • Molecular Biology (AREA)
  • Zoology (AREA)
  • Nutrition Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Non-Alcoholic Beverages (AREA)
US05/944,697 1977-10-19 1978-09-22 Methods for making flocculation-resistant citrus juice Expired - Lifetime US4211799A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE274688 1977-10-19
DE2746884A DE2746884C2 (de) 1977-10-19 1977-10-19 Verfahren zur Herstellung von klarem oder trübem, flockungsbeständigem Citrussaft

Publications (1)

Publication Number Publication Date
US4211799A true US4211799A (en) 1980-07-08

Family

ID=6021750

Family Applications (1)

Application Number Title Priority Date Filing Date
US05/944,697 Expired - Lifetime US4211799A (en) 1977-10-19 1978-09-22 Methods for making flocculation-resistant citrus juice

Country Status (6)

Country Link
US (1) US4211799A (de)
AR (1) AR215749A1 (de)
DE (1) DE2746884C2 (de)
ES (1) ES473913A1 (de)
IL (1) IL55632A0 (de)
IT (1) IT1108169B (de)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5112627A (en) * 1990-01-19 1992-05-12 O.M.C. Officina Meccanica Collareda S.R.L Stabilization process particularly for grape must
EP1013179A1 (de) * 1998-12-27 2000-06-28 Dsm N.V. Klärung von Fruchtsäften
WO2001076609A1 (de) * 2000-04-06 2001-10-18 Technische Universität Berlin Herstellung von polygalakturoniden und ihre verwendung als lebensmittelzusatzstoffe
KR100386704B1 (ko) * 2000-10-06 2003-06-02 우강융 유자주스 및 그 제조방법
US20050008734A1 (en) * 2003-07-03 2005-01-13 Westphal Kathleen A. Nutritious strawberry fruit juice drink and method of making the same
WO2005070234A1 (en) * 2003-12-23 2005-08-04 Council Of Scientific And Industrial Research Process for the production of sediment free clarified fruit juices
KR20050099902A (ko) * 2004-04-12 2005-10-17 학교법인 영광학원 청징 및 농축에 의한 오렌지주스의 제조방법
US20060246201A1 (en) * 2002-11-29 2006-11-02 Council Of Scientific And Industrial Research Of Insdoc Building Process for preparation of shelf stable fruit spread with no added sugar

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3221576A1 (de) * 1982-06-08 1983-12-08 Röhm GmbH, 6100 Darmstadt Verfahren zum verfluessigen von obst- und gemuesemaischen und -saeften
DE3304437C2 (de) * 1983-01-31 1985-05-09 Karl Dr. 8000 München Raible Verfahren zur Behandlung von Würze oder Bier unter Anwendung von Kieselsol

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3754932A (en) * 1971-04-16 1973-08-28 Us Agriculture Proteare and pectmare additive to citrus juices
US4109017A (en) * 1976-02-25 1978-08-22 Rohm Gmbh Method for clarification of fruit juice

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE649164C (de) * 1933-12-22 1937-08-17 I G Farbenindustrie Akt Ges Verfahren zum Klaeren von rohen Fruchtsaeften, Suessmosten, und aehnlichen Erzeugnissen

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3754932A (en) * 1971-04-16 1973-08-28 Us Agriculture Proteare and pectmare additive to citrus juices
US4109017A (en) * 1976-02-25 1978-08-22 Rohm Gmbh Method for clarification of fruit juice

Non-Patent Citations (7)

* Cited by examiner, † Cited by third party
Title
Chemical Abstract, 81 48770a. *
Endo, Agr. Biol. Chem. 28, 535-542 (1965). *
Enzyme Topics, No. 3, May 1964, Rohm and Haas Co., _Phila., Pa. (pp. 1-4). *
Food Science and Technology Abstracts (FSTA) vol. 3, Section 1 (1971). *
Hultin et al., Archives of Biochem & Biophysics, 101, 396-402 (1963). *
Purr et al., Biochemiche Zeitschrift, 329, 261-273 (1957). *
Rohm and Haas Company data sheet on Pectinol 41-P concentrate. *

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5112627A (en) * 1990-01-19 1992-05-12 O.M.C. Officina Meccanica Collareda S.R.L Stabilization process particularly for grape must
US6355284B1 (en) 1998-12-27 2002-03-12 Dsm N.V. Fruit juice clarification
EP1013179A1 (de) * 1998-12-27 2000-06-28 Dsm N.V. Klärung von Fruchtsäften
US20040146635A1 (en) * 2000-04-06 2004-07-29 Technische Universitat Berlin Production of polygalacturonides and their use in food additives
US6696554B2 (en) * 2000-04-06 2004-02-24 Technische Universitat Berlin Production of polygalacturonides and their use as food additives
WO2001076609A1 (de) * 2000-04-06 2001-10-18 Technische Universität Berlin Herstellung von polygalakturoniden und ihre verwendung als lebensmittelzusatzstoffe
KR100386704B1 (ko) * 2000-10-06 2003-06-02 우강융 유자주스 및 그 제조방법
US20060246201A1 (en) * 2002-11-29 2006-11-02 Council Of Scientific And Industrial Research Of Insdoc Building Process for preparation of shelf stable fruit spread with no added sugar
US20050008734A1 (en) * 2003-07-03 2005-01-13 Westphal Kathleen A. Nutritious strawberry fruit juice drink and method of making the same
WO2005006879A2 (en) * 2003-07-03 2005-01-27 California Giant, Inc. Nutritious strawberry fruit juice drink and method of making the same
WO2005006879A3 (en) * 2003-07-03 2006-01-12 California Giant Inc Nutritious strawberry fruit juice drink and method of making the same
US7037539B2 (en) * 2003-07-03 2006-05-02 California Giant, Inc. Nutritious strawberry fruit juice drink and method of making the same
WO2005070234A1 (en) * 2003-12-23 2005-08-04 Council Of Scientific And Industrial Research Process for the production of sediment free clarified fruit juices
KR20050099902A (ko) * 2004-04-12 2005-10-17 학교법인 영광학원 청징 및 농축에 의한 오렌지주스의 제조방법

Also Published As

Publication number Publication date
AR215749A1 (es) 1979-10-31
IL55632A0 (en) 1978-12-17
IT1108169B (it) 1985-12-02
IT7869252A0 (it) 1978-09-29
DE2746884C2 (de) 1985-03-07
ES473913A1 (es) 1979-04-01
DE2746884A1 (de) 1979-04-26

Similar Documents

Publication Publication Date Title
Domingues et al. Clarification of passion fruit juice with chitosan: Effects of coagulation process variables and comparison with centrifugation and enzymatic treatments
DE69937062T2 (de) Verfahren zur isolierung einer beta-glucan-zusammensetzung aus hafer sowie daraus hergestellte produkte
US6428837B1 (en) Deesterified pectins, processes for producing such pectins, and stabilized acidic liquid systems comprising the same
US4211799A (en) Methods for making flocculation-resistant citrus juice
KR100371475B1 (ko) 차 추출액의 효소적 청징화법
US20080081094A1 (en) Processed mango juice and beverage containing it
EP0562171A2 (de) Wasserlösliche Polysaccharide und Verfahren zu ihrer Herstellung
JP2000273101A (ja) ペクチン及びその製造法並びにそれを使用した酸性蛋白食品及びその製造法
US3917867A (en) Process for producing a natural orange base by dilution and centrifuging
HU220375B (hu) Eljárás ivólevek és pektintartalmú törköly, és az utóbbiból pektin előállítására, és az így kapott termékek
Endo Studies on Pectolytic Enzymes of Molds: Part XIII. Clarification of Apple Juice by the Joint Action of Purified Pectolytic EnzymesPart XIV. Properties of Pectin in Apple Juice
US4109017A (en) Method for clarification of fruit juice
US4327115A (en) Clarification of fruit juice with honey
US4101678A (en) Clarification of citrus juices
JP2002272429A (ja) 甘藷飲料
BAKER Clarification of citrus juices with polygalacturonic acid
JPS6341548B2 (de)
JPS6339564A (ja) 植物部分から調製した液体の清澄化方法
WO2021193414A1 (ja) 大豆原料の加熱処理物及びそれを有効成分とする起泡剤
JPS58186491A (ja) ミカン缶詰廃液の処理方法及びミカン缶詰廃液からペクチン質を製造する方法
US6355284B1 (en) Fruit juice clarification
JP3181428B2 (ja) 飲 料
JP2000157175A (ja) 果汁入り紅茶飲料
JP2920382B2 (ja) 果汁等成分の分離法と分離された有用成分物質及び分離された有用成分物質の製造法
JP3579597B2 (ja) 茶飲料